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1.
A cloud point extraction procedure for the preconcentration of copper, nickel, iron and zinc ions in various samples has been described. Analyte ions in aqueous phase are complexed with 3-((indolin-3-yl)(phenyl)methyl)indoline (IYPMI) and following centrifugation quantitatively extracted to the aqueous phase rich in Triton X-114. The surfactant-rich phase was dissolved in 2.0 mol L−1 HNO3 in methanol prior to metal content determination by flame atomic absorption spectrometry (FAAS). The effects of some parameters including, the concentrations of IYPMI, Triton X-114 and HNO3, bath temperature, centrifuge rate and time were investigated on the recoveries of analyte ions. At optimum conditions, the detection limits of (3 SDb m−1) of 1.6, 2.8, 2.1 and 1.1 ng mL−1 for Cu2+, Fe3+, Ni2+ and Zn2+ along with preconcentration factors of 30 and enrichment factor of 48, 39, 34 and 52 for Cu2+, Ni2+, Fe3+ and Zn2+ respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as biological, soil and blood samples with high efficiency.   相似文献   

2.
A method for the simultaneous preconcentration of Cu2+,Zn2+ and Fe3+ ions, in some food samples has been reported. The method is based on the adsorption of 3‐(1‐(1‐H‐indol‐3‐yl)‐3‐phenylallyl)‐1H‐indole (IPAI) loaded on Duolite XAD 761. The metal ions adsorbed on the modified solid phase resin are eluted using 6 mL of 4 mol L?1 nitric acid. The influences of the analytical parameters including pH and amount of ligand and solid phase and type and amount of surfactant and sample volume on the metal ions recoveries were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally higher than 95% with a RSD lower than 5%. The method has been successfully applied for these metals content evaluation in some real samples.  相似文献   

3.
The Amberlite XAD-7 resin modification was carried out by loading 2-(1-(4-chlorophenyl)-4,5-diphenyl-1H-imidazol-2yl)-4-nitrophenol (CPDPINP). Subsequently, this new sorbent was applied for the enrichment of metal ions such as Cu2+, Ni2+, Co2+ Zn2+ and Pb2+ ions. The effect of various parameters on their sorption and following recoveries was studied in column procedure. The preconcentrated ions were eluted by appropriate eluent and their contents were quantified by FAAS. This method has preconcentration factor of 150 and enrichment factor in the range of 20.8–29.1. At optimum values of all variables, the proposed method has linear calibration graphs in the range of 0.01 up to 0.29 μg mL−1 with detection limit (3SDb/m, n = 15) between 1.6 and 2.6 ng mL−1. This protocol is usable for successful analysis of Cu2+, Ni2+, Co2+ Zn2+ and Pb2+ ions in different matrices with reasonable recoveries (>93%) and acceptable relative standard deviation (<4.7%).  相似文献   

4.
Three coordination polymers (CPs) based on the 5‐[4‐(1H‐imidazol‐1‐yl)phenyl]‐1H‐tetrazole ( HL ) ligand, namely, [Cu(μ2‐ L )(μ4‐pbda)(H2O)] ( 1 ), [Cu2(μ‐Hbtc)(H2btc)(μ3‐OH)(μ4‐ HL )] ( 2 ) and [Cu53‐ L )(μ4‐ L )(μ3‐ip)(μ3‐OH)(H2O)2] · 2H2O ( 3 ) (H2pbda = 1,4‐benzenedicarboxylic acid, H3btc = 1,3,5‐benzenetricarboxylic acid, H2ip = isophthalic acid) were hydrothermally synthesized and structurally characterized. Complex 1 represents “weave”‐type 2D layers consisting of wave‐like 1D chains and 1D straight chains, which are further connected by hydrogen bonds to form a 3D supramolecular structure. Complex 2 exhibits a uninodal (4)‐connected 2D layer with a point symbol of {44 · 62}, in which the L ligand can be described as μ5‐bridging and the H2btc ions display multiple kinds of coordination modes to connect CuII ions into 1D “H”‐type Cu‐H2btc chains. In complex 3 , 2D Cu‐ L layers with two kinds of grids and 1D “stair”‐type Cu‐ip chains link each other to construct a 3D {412 · 63} framework, which contains the pentanuclear subunits. Deprotonated degree and coordination modes of carboxylate ligands may consequentially influence the coordination patterns of main ligands and the final structures of complexes 1 – 3 . Furthermore, electrochemical behaviors and electrocatalytic activities of the title complexes were analyzed at room temperature, suggesting practical applications in areas of electrocatalytic reduction toward nitrite and hydrogen dioxide in aqueous solutions, respectively.  相似文献   

5.
A new chelating resin containing bis[2-(2-benzothiazolylthioethyl)sulfoxide] was synthesized using chloromethylated polystyrene as material and characterized by elemental analysis and infrared spectra. The adsorption capacities of the newly formed resin for Hg2+, Ag+, Cu2+, Zn2+, Pb2+, Mn2+, Ni2+, Cd2+ and Fe3+ were investigated over the pH range 1.0-6.0. The resin exhibited no affinity for alkali or alkaline earth metal ions. The maximum adsorption capacities of the resin for Hg2+, Ag+, Cu2+, Zn2+, Pb2+, Mn2+, Ni2+, Cd2+ and Fe3+ were 1.49, 0.96, 0.58, 0.11, 0.37, 0, 0.24, 0.36 and 0.25 mmol g−1, respectively. In column operation it had been observed that Hg2+ and Ag+ in trace quantity could be separated from different binary mixtures and Hg2+ could be effectively removed from industrial wastewater and the natural water spiked with Hg2+ at usual pH.  相似文献   

6.
Solvent extraction of a mixture of PbII, MnII, FeIII, CoII, NiII and CdII in aqueous perchlorate medium by a phosphorylated hexahomotrioxacalix[3]arene (calix‐3) in dichloromethane shows a significant selectivity towards lead ions. The ligand can also be incorporated into a membrane to provide a new lead ion‐selective electrode (PbII‐ISE). A plasticized PVC membrane containing 30% PVC, 53.5% ortho‐nitrophenyloctylether (NPOE), 4.5% sodium tetraphenylborate (NaTPB) and 12% ionophore was directly coated on a graphite rod. This sensor gave a good Nernstian response of 29.7 ± 0.7 mV decade?1 over a concentration range of 1 × 10?8 – 1 × 10?4 M of lead ions, independent of pH in the range 3‐7, with a detection limit of 0.4 × 10?8 M. The dynamic response time of the electrode to achieve a steady potential was very fast and found to be less than 7 s. The selectivity relative to Ag+, NH4+, Li+, Na+, K+, Ca2+, Sr2+, Ba2+, Mn2+, Fe2+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Fe3+, La3+, Sm3+, Dy3+, Er3+, Y3+ and Th4+ was examined. The electrode exhibits adequate stability with good reproducibility (with a slope of 29.6 ± 1.5 mV for 8 weeks). The characteristics of the sensor are compared with those of a tetraphosphorylated calix[4]arene (calix‐4) based PbII‐ISE, reported recently. The electrode was successfully used as an indicator electrode for a potentiometric titration of a lead solution using a standard solution of EDTA. The applicability of the sensor for lead ion measurements in various synthetic samples was also investigated.  相似文献   

7.
The Fe3+ ion is the most important element in environmental systems and plays a fundamental role in biological processes. Iron deficiency can result in diseases and highly selective and sensitive detection of trace Fe3+ has become a hot topic. A novel two‐dimensional ZnII coordination framework, poly[[μ‐4,4′‐bis(2‐methylimidazol‐1‐yl)diphenyl ether‐κ2N3:N3′](μ‐4,4′‐sulfonyldibenzoato‐κ2O:O′)zinc(II)], [Zn(C14H8O6S)(C20H18N4O)]n or [Zn(SDBA)(BMIOPE)]n, (I), where H2SDBA is 4,4′‐sulfonyldibenzoic acid and BMIOPE is 4,4′‐bis(2‐methylimidazol‐1‐yl)diphenyl ether, has been prepared and characterized by IR, elemental analysis, thermal analysis and X‐ray diffraction analysis, the latter showing that the coordination polymer exhibits a threefold interpenetrating two‐dimensional 44‐ sql network. In addition, it displays a highly selective and sensitive sensing for Fe3+ ions in aqueous solution.  相似文献   

8.
The efficiencies and performances of silver nanoparticle loaded activated carbon modified with 2-(4-isopropylbenzylideneamino)thiophenol (IPBATP-Ag-NP-AC) and activated carbon modified with IPBATP (IPBATP-AC), as new sorbents, were evaluated for separation and preconcentration of Cu2+, Zn2+, Co2+, Cd2+ and Pb2+ ions from real environmental samples. The retained metals content was reversibly eluted using 5?mL of CH3COOH (6.0?mol?L?1) and/or 10?mL of 4.0?mol?L?1 HNO3 for IPBATP-Ag-NP-AC and IPBATP-AC, respectively. The experimental parameters influence the recoveries of metal ions including pH, amounts of ligand and supports, condition of eluents, sample and eluent flow rates of has been investigated. The preconcentration factors were found to be 100 for Zn2+, Cd2+, Co2+, Cu2+ and 50 for Pb2+ ions using IPBATP-Ag-NP-AC, and 50 for Zn2+, Cd2+, Co2+, Cu2+ and 25 for Pb2+ ions using IPBATP-AC. The detection limit of both SPE-based sorbents was between 1.6–2.5?ng?mL?1 for IPBATP-AC and 1.3–2.5?ng?mL?1 for IPBATP-Ag-NP-AC. The proposed methods have been successfully applied for the extraction and determination of the understudy metal ions content in some real samples with extraction efficiencies higher than 90% and relative standard deviations (RSD) lower than 2.4%.  相似文献   

9.
The bis-{N-(2-hydroxynaphthyl-1-methylimine)} anchored 1,3-di-derivative of lower rim p-tert-butyl-calix[4]arene possessing a N2O2, N2O4 or N2O6 binding core was found to be selective for Zn(II) ions even at ?60 ppb by eliciting fluorescence-on behaviour while the other ions, viz., Ti4+, VO2+, Cr3+, Mn2+, Fe2+, Co2+, Ni2+, Cu2+, Mg2+, Cd2+ and Hg2+ caused no change in the fluorescence. The reaction between 1 and Zn2+ was found to be stoichiometric with the formation of a 1:1 complex; while H+ quenched the fluorescence of the complex, OH restored it. The studies of the 1:1 isolated complexes of Zn2+, Ni2+ and Cu2+ augmented the results.  相似文献   

10.
A new glucose-based C2-derivatized colorimetric chemo-sensor (L1) has been synthesized by a one-step condensation of glucosamine and 2-hydroxy-1-naphthaldehyde for the recognition of transition metal ions. Among the eleven metal ions studied, viz., Mg2+, Ca2+, Mn2+, Fe2+, Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+ and Hg2+, L1 results in visual colour change only in the presence of Fe2+, Fe3+and Cu2+ in methanol. However, in an aqueous HEPES buffer (pH 7.2) it is only the Fe3+ that gives a distinct visual colour change even in the presence of other metal ions, up to a concentration of 280 ppb. The changes have been explained based on the complex formed, and the composition has been determined to be 2:1 between L1 and Fe3+ based on Job’s plot as well as ESI MS. The structure of the proposed complex has been derived based on HF/6-31G calculations.  相似文献   

11.
The complex poly[[aqua(μ2‐phthalato‐κ2O1:O2){μ3‐2‐[3‐(pyridin‐2‐yl)‐1H‐pyrazol‐1‐yl]acetato‐κ4N2,N3:O:O′}{μ2‐2‐[3‐(pyridin‐2‐yl)‐1H‐pyrazol‐1‐yl]acetato‐κ3N2,N3:O}dizinc(II)] dihydrate], {[Zn2(C10H8N3O2)2(C8H4O4)(H2O)]·2H2O}n, has been prepared by solvothermal reaction of 2‐[3‐(pyridin‐2‐yl)‐1H‐pyrazol‐1‐yl]acetonitrile (PPAN) with zinc(II). Under hydrothermal conditions, PPAN is hydrolyzed to 2‐[3‐(pyridin‐2‐yl)‐1H‐pyrazol‐1‐yl]acetate (PPAA). The structure determination reveals that the complex is a one‐dimensional double chain containing cationic [Zn4(PPAA)4]4+ structural units, which are further extended by bridging phthalate ligands. The one‐dimensional chains are extended into a three‐dimensional supramolecular architecture via hydrogen‐bonding and π–π stacking interactions.  相似文献   

12.
《Electroanalysis》2006,18(10):1019-1027
A new PVC membrane potentiometric sensor for Ag(I) ion based on a recently synthesized calix[4]arene compound of 5,11,17,23‐tetra‐tert‐butyl‐25,27‐dihydroxy‐calix[4]arene‐thiacrown‐4 is developed. The electrode exhibits a Nernstian response for Ag(I) ions over a wide concentration range (1.0×10?2?1.0×10?6 M) with a slope of 53.8±1.6 mV per decade. It has a relatively fast response time (5–10 s) and can be used for at least 2 months without any considerable divergence in potentials. The proposed electrode shows high selectivity towards Ag+ ions over Pb2+, Cd2+, Co2+, Zn2+, Cu2+, Ni2+, Sr2+, Mg2+, Ca2+, Li+, K+, Na+, NH4+ ions and can be used in a pH range of 2–6. Only interference of Hg2+ is found. It is successfully used as an indicator electrode in potentiometric titration of a mixture of chloride, bromide and iodide ions.  相似文献   

13.
Rigid N‐(substituted)‐2‐aza‐[3]‐ferrocenophanes L1 and L2 were easily synthesized from 1,1 ‐dicarboxyaldehydeferrocene and the corresponding amines. Ligands L1 and L2 were characterized by 1H NMR, 13C NMR and single‐crystal X‐ray crystallography. The coordination abilities of L1 and L2 with metal ions such as Cu2+, Mg2+, Ni2+, Zn2+, Pb2+ and Cd2+ were evaluated by cyclic voltammetry. The electrochemical shift (ΔE1/2) of 125 mV was observed in the presence of Cu2+ ion, while no significant shift of the Fc/Fc + couple was observed when Mg2+, Ni2+, Zn2+, Pb2+, Cd2+ metal ions were added to the solution of L1 in the mixture of MeOH and H2O. Moreover, the extent of the anodic shift of redox potentials was approximately equal to that induced by Cu2+ alone when a mixture of Cu2+, Mg2+, Ni2+, Zn2+, Pb2+ and Cd2+ was added to a solution of L1. Ligand L1 was proved to selectively sense Cu2+ in the presence of large, excessive first‐row transition and late‐transition metal cations. The coordination model was proposed from the results of controlled experiments and quantum calculations. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

14.
Multiwalled carbon nanotubes chemically functionalized with 2-((3-silylpropylimino) methyl) phenol (SPIMP-MWCNT) and successfully applied for the solid phase extraction (SPE) of some metal ions in food samples. The influences of the analytical parameters including pH, amounts of solid phase, eluent conditions (type, volume and concentrations), sample volume and interference of some metal ions on the recoveries of ions Cu2+, Pb2+, Fe2+, Ni2+ and Zn2+ ion were investigated. The metal ions retained on SPIMP-MWCNT was eluted using 6?mL of 4?mol?L?1 HNO3 solution and their content was determined by flame atomic absorption spectrometry (FAAS) with recoveries more than 95% and relative standard deviations (n?=?5) between 2.4–3.4% for both reproducibility and repeatability. The detection limit of this metal ions was between 1.0–2.6?ng?mL?1 (3S b , n?=?10) and their preconcentration factor was 100, while their loading capacity was above 32.9?mg?g?1 of SPIMP-MWCNT. The proposed method was successfully applied for the preconcentration and determination of analytes in different samples.  相似文献   

15.
A new ratiometric fluorescent sensor ( 1 ) for Cu2+ based on 4,4‐difluoro‐4‐bora‐3a,4a‐diaza‐s‐indacene (BODIPY) with di(2‐picolyl)amine (DPA) as ion recognition subunit has been synthesized and investigated in this work. The binding abilities of 1 towards different metal ions such as alkali and alkaline earth metal ions (Na+, K+, Mg2+, Ca2+) and other metal ions ( Ba2+, Zn2+, Cd2+, Fe2+, Fe3+, Pb2+, Ni2+, Co2+, Hg2+, Ag+) have been examined by UV‐vis and fluorescence spectroscopies. 1 displays high selectivity for Cu2+ among all test metal ions and a ~10‐fold fluorescence enhancement in I582/I558 upon excitation at visible excitation wavelength. The binding mode of 1 and Cu2+ is a 1:1 stoichiometry determined via studies of Job plot, the nonlinear fitting of the fluorometric titration and ESI mass.  相似文献   

16.
A new porous solid macrocyclic 1,4,7,10,14,17,20‐heptaazadocosane‐3,21‐dione polysiloxane ligand system of the general formula P‐(CH2)3‐C15H32O2N5, (where P represents [Si‐O]n siloxane network) has been prepared by the reaction of immobilized iminobis(N‐diethylenediamineacetamide)polysiloxane with 1,3 dibromopropane. The new macrocyclic polysiloxane ligand system exhibits high potential for the uptake of metal ions (Fe3+, Co2+, Ni2+, Cu2+ and Zn2+). Complexation with copper ions exhibits a high selectivity in which two copper ions were involved per one macrocyclic ligand group.  相似文献   

17.
Two isostructural heterometallic complexes, {[Dy3Ni3(H2O)3(mpko)9(O2)(NO3)3](ClO4) · 3CH3OH · 3CH3CN} ( 1 ) and {[Gd3Ni3(H2O)3(mpko)9(O2)(NO3)3](NO3) · 10.75CH3OH} ( 2 ) [mpkoH = 1‐(pyrazin‐2‐yl)ethanone oxime], were solvothermally synthesized by varying lanthanide ions with different magnetic anisotropy. Structural analyses revealed that both complexes contain a peroxide anion‐aggregated triangular {Ln33‐Ο2)}7+ core, which is surrounded by three NiII octahedra through threefold oxime linkages into a heterometallic hexanuclear cluster. Apparent antiferromagnetic interactions are observed between the adjacent spin carriers of 1 and 2 with the coupling constant JLn ··· Ni ≈ 12JLn ··· Ln. Additionally, 1 with highly anisotropic DyIII site shows slow magnetization relaxation under zero dc field and 2 constructed from isotropic GdIII ion displays significant cryogenic magnetocaloric effect with a maximum entropy change of 24.8 J · kg–1 · K–1 at 3.0 K and 70 kOe.  相似文献   

18.
A method for solid phase extraction of trace metals such as Cd2+, Cr6+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+ using nanometer-sized alumina coated with chromotropic acid prior to determination by inductively coupled plasma atomic emission spectrometry (ICP-AES) has been developed. Various influencing parameters on the separation and preconcentration of trace metals, pH, flow rate, sample volume, amount of adsorbent, concentration of eluent and sorption kinetics have been studied. The detection limits for Cd2+, Cr6+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+ were found to be 0.14, 0.62, 0.22, 0.54, 0.27, 0.28, 0.53 and 0.38 ng ml− 1, respectively. The adsorption capacity of the solid phase adsorption material is 10.3, 11.3, 14.5, 16.4, 15.1, 11.7, 15.4 and 16.8 mg g− 1 for Cd2+, Cr6+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+, respectively. The preconcentration factor was obtained in the range of 50-100 for all studied metal ions. Coexisting ions over a high concentration range have not shown any significant effects on the determination of aforesaid metal ions. The accuracy of the proposed method was tested by standard reference materials (NIST 1643e: water, NIST 1573a: tomato leaves and NIST 1568a rice flour) and natural waters and the results obtained were in good agreement with the certified values.  相似文献   

19.
Trace amounts of Fe3+, Pb2+, Cu2+, Ni2+, Co2+ and Zn2+ ions were efficiently enriched following complexation with silica-gel chemically functionalized with 2-((3-silylpropylimino)methyl)-5-bromophenol. The enriched metal ions efficiently eluted with 6?mL of 4.0?mol?L?1 nitric acid and their metal contents were determined by flame atomic absorption spectrometry (FAAS). The influences of the analytical parameters and experimental variables on the recoveries of the metal ions under study were investigated and optimized. The method has high sorption preconcentration efficiency even in the presence of various interfering ions. At optimum values of all variables the method is applicable for analysis of real samples with recoveries in the range of 95 to 105% with RSD lower than 4.2% and detection limits between 1.4 and 2.8?µg?L?1.  相似文献   

20.
A long wavelength emission fluorescent (612 nm) chemosensor with high selectivity for H2PO4? ions was designed and synthesized according to the excited state intramolecular proton transfer (ESIPT). The sensor can exist in two tautomeric forms ('keto' and 'enol') in the presence of Fe3+ ion, Fe3+ may bind with the 'keto' form of the sensor. Furthermore, the in situ generated GY‐Fe3+ ensemble could recover the quenched fluorescence upon the addition of H2PO4? anion resulting in an off‐on‐type sensing with a detection limit of micromolar range in the same medium, and other anions, including F?, Cl?, Br?, I?, AcO?, HSO4?, ClO4? and CN? had nearly no influence on the probing behavior. The test strips based on 2‐[2‐hydroxy‐4‐(diethylamino) phenyl]‐1H‐imidazo[4,5‐b]phenazine and Fe3+ metal complex ( GY‐Fe3+ ) were fabricated, which could act as convenient and efficient H2PO4? test kits.  相似文献   

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